US20110143916A1 - Catalyst production method and system - Google Patents
Catalyst production method and system Download PDFInfo
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- US20110143916A1 US20110143916A1 US12/965,745 US96574510A US2011143916A1 US 20110143916 A1 US20110143916 A1 US 20110143916A1 US 96574510 A US96574510 A US 96574510A US 2011143916 A1 US2011143916 A1 US 2011143916A1
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- catalyst support
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- catalytic particles
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- 239000003054 catalyst Substances 0.000 title claims abstract description 101
- 238000004519 manufacturing process Methods 0.000 title 1
- 238000000034 method Methods 0.000 claims abstract description 104
- 239000002245 particle Substances 0.000 claims abstract description 95
- 239000006185 dispersion Substances 0.000 claims abstract description 80
- 230000003197 catalytic effect Effects 0.000 claims abstract description 70
- 239000002904 solvent Substances 0.000 claims abstract description 47
- 238000009826 distribution Methods 0.000 claims abstract description 27
- 238000002156 mixing Methods 0.000 claims abstract description 20
- 239000002244 precipitate Substances 0.000 claims abstract description 15
- 238000004458 analytical method Methods 0.000 claims abstract description 9
- 239000011877 solvent mixture Substances 0.000 claims description 48
- 239000000843 powder Substances 0.000 claims description 40
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 claims description 29
- 238000001035 drying Methods 0.000 claims description 25
- 238000005470 impregnation Methods 0.000 claims description 22
- 238000002296 dynamic light scattering Methods 0.000 claims description 16
- 238000001354 calcination Methods 0.000 claims description 10
- 238000004108 freeze drying Methods 0.000 claims description 10
- 238000000527 sonication Methods 0.000 claims description 4
- 239000011858 nanopowder Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 abstract description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- 239000007788 liquid Substances 0.000 description 10
- 238000011068 loading method Methods 0.000 description 9
- 239000000463 material Substances 0.000 description 9
- 229910052757 nitrogen Inorganic materials 0.000 description 6
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- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000010970 precious metal Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000000921 elemental analysis Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- 102000002322 Egg Proteins Human genes 0.000 description 1
- 108010000912 Egg Proteins Proteins 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 210000003278 egg shell Anatomy 0.000 description 1
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- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- 238000003913 materials processing Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910052756 noble gas Inorganic materials 0.000 description 1
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- SYQBFIAQOQZEGI-UHFFFAOYSA-N osmium atom Chemical compound [Os] SYQBFIAQOQZEGI-UHFFFAOYSA-N 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- -1 platinum group metals Chemical class 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
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- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Images
Classifications
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
- B01J37/0211—Impregnation using a colloidal suspension
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/8926—Copper and noble metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/42—Platinum
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/009—Preparation by separation, e.g. by filtration, decantation, screening
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/32—Freeze drying, i.e. lyophilisation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/349—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of flames, plasmas or lasers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J6/00—Heat treatments such as Calcining; Fusing ; Pyrolysis
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B23/00—Arrangements specially adapted for the production of shaped articles with elements wholly or partly embedded in the moulding material; Production of reinforced objects
- B28B23/0081—Embedding aggregates to obtain particular properties
- B28B23/0087—Lightweight aggregates for making lightweight articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/14—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
- C23C4/134—Plasma spraying
Definitions
- the present invention relates to the field of catalysts. More specifically, the present invention relates to a method of producing a catalyst.
- a method of producing a catalyst comprises mixing a plurality of catalytic particles and a solvent, thereby forming a particle-solvent mixture.
- a size distribution analysis is performed on a sample of the particle-solvent mixture, thereby determining a size distribution profile for the particle-solvent mixture.
- the mixing of the catalytic particles and the solvent in the particle-solvent mixture is repeated if the size distribution profile is below a predetermined threshold.
- the entire particle-solvent mixture is centrifuged if the size distribution profile is at or above the predetermined threshold, thereby forming a supernate of the particle-solvent mixture and a precipitate of the particle-solvent mixture within the same container, wherein the supernate comprises a dispersion including the catalytic particles and the solvent.
- the particle-solvent mixture is decanted, thereby separating the supernate from the precipitate.
- the particle content of a sample of the separated supernate is determined.
- a target volume of the dispersion to be applied to a catalyst support is determined based on one or more properties of the catalyst support.
- the catalyst support is impregnated with the catalytic particles in the dispersion by applying the target volume of the dispersion to the catalyst support.
- the method further comprises the step of calcining the impregnated catalyst support. In some embodiments, the method further comprises the step of performing a drying process on the impregnated catalyst support before the step of calcining the impregnated catalyst support. In some embodiments, the drying process is a freeze drying process.
- the method further comprises the step of analyzing the impregnated catalyst support to determine if it has been sufficiently impregnated according to one or more predetermined thresholds.
- the step of analyzing the impregnated catalyst support comprises performing an Inductively Coupled Plasma Mass Spectrometry (ICP-MS) process on the impregnated catalyst support.
- the method further comprises the step of performing an additional impregnation of the impregnated catalyst support with a dispersion of catalytic particles in response to a determination by the analyzing step that the impregnated catalyst support has not been sufficiently impregnated according to the one or more thresholds.
- ICP-MS Inductively Coupled Plasma Mass Spectrometry
- the catalyst support is a porous extrudate. In some embodiments, the catalyst support is a monolith. In some embodiments, the catalyst support is a powder.
- the step of mixing the plurality of catalytic particles and the solvent comprises using a shear mixer to mix the plurality of catalytic particles and the solvent. In some embodiments, the step of mixing the plurality of catalytic particles and the solvent comprises using sonication to mix the plurality of catalytic particles and the solvent.
- the step of performing a size distribution analysis on the sample of the particle-solvent mixture comprises: centrifuging the sample of the particle-solvent mixture; and performing a Dynamic Light Scattering (DLS) process on the centrifuged sample.
- DLS Dynamic Light Scattering
- the step of determining the particle content of the sample of the separated supernate comprises calculating the weight percentage of the catalytic particles in the sample. In some embodiments, the step of determining the particle content of the sample of the separated supernate comprises performing an Inductively Coupled Plasma Mass Spectrometry (ICP-MS) process on the sample.
- ICP-MS Inductively Coupled Plasma Mass Spectrometry
- the plurality of catalytic particles that is mixed with the solvent is a nano-powder.
- a method of producing a catalyst comprises mixing a plurality of catalytic particles and a solvent, thereby forming a particle-solvent mixture.
- a sample of the particle-solvent mixture is centrifuged.
- a Dynamic Light Scattering (DLS) process is performed on the centrifuged sample, thereby determining a size distribution profile for the particle-solvent mixture.
- the mixing of the catalytic particles and the solvent in the particle-solvent mixture is repeated if the size distribution profile is below a predetermined threshold.
- the entire particle-solvent mixture is centrifuged if the size distribution profile is at or above the predetermined threshold, thereby forming a supernate of the particle-solvent mixture and a precipitate of the particle-solvent mixture within the same container, wherein the supernate comprises a dispersion including the catalytic particles and the solvent.
- the particle-solvent mixture is decanted, thereby separating the supernate from the precipitate.
- the catalyst support is impregnated with the catalytic particles in the dispersion by applying a volume of the dispersion to the catalyst support.
- the method further comprises performing a dry-down process on a sample of the separated dispersion, and performing a weight percentage calculation of the catalytic particles using the dried-down sample of the separated dispersion, thereby determining a weight percentage for the catalytic particles.
- the step of impregnating the catalyst support is performed only if the determined weight percentage for the catalytic particles is at or above a predetermined threshold.
- an Inductively Coupled Plasma Mass Spectrometry (ICP-MS) process is performed on the dried-down sample of the separated dispersion.
- ICP-MS Inductively Coupled Plasma Mass Spectrometry
- a method of producing a catalyst comprises providing a dispersion, wherein the dispersion comprises catalytic particles dispersed in a solvent.
- a target volume of the dispersion to be applied to a catalyst support is determined based on one or more properties of the catalyst support.
- the catalyst support is impregnated with the catalytic particles in the dispersion by applying the target volume of the dispersion to the catalyst support.
- a drying process is performed on the impregnated catalyst support. The dried impregnated catalyst support is calcined.
- ICP-MS Inductively Coupled Plasma Mass Spectrometry
- the catalyst support is a porous extrudate. In some embodiments, the catalyst support is a monolith. In some embodiments, the catalyst support is a powder.
- the drying process is a freeze drying process. In some embodiments, the drying process is either a hot drying process or a flash drying process.
- FIG. 1 illustrates one embodiment of a method of producing a catalyst in accordance with the principles of the present invention.
- FIG. 2A illustrates one embodiment of a method of producing a dispersion in accordance with the principles of the present invention.
- FIG. 2B illustrates one embodiment of a method of impregnating a catalyst support with particles from a dispersion in accordance with the principles of the present invention.
- Powders that fall within the scope of the present invention may include, but are not limited to, any of the following: (a) nano-structured powders (nano-powders), having an average grain size less than 250 nanometers and an aspect ratio between one and one million; (b) submicron powders, having an average grain size less than 1 micron and an aspect ratio between one and one million; (c) ultra-fine powders, having an average grain size less than 100 microns and an aspect ratio between one and one million; and (d) fine powders, having an average grain size less than 500 microns and an aspect ratio between one and one million.
- nano-powders nano-structured powders
- submicron powders having an average grain size less than 1 micron and an aspect ratio between one and one million
- ultra-fine powders having an average grain size less than 100 microns and an aspect ratio between one and one million
- fine powders having an average grain size less than 500 microns and an aspect ratio between one and one million.
- FIG. 1 illustrates one embodiment of a method 100 of producing a catalyst in accordance with the principles of the present invention.
- a plurality of catalytic particles and a solvent are mixed together, thereby forming a particle-solvent mixture.
- the catalytic particles can be made up of any particles having catalytic properties such that they modify, either by increasing or decreasing, the rate of a chemical reaction.
- the catalytic particles comprise or consist of one or more precious metals.
- the catalytic particles comprise one of the platinum group metals, such as ruthenium, rhodium, palladium, osmium, iridium, and platinum.
- platinum group metals such as ruthenium, rhodium, palladium, osmium, iridium, and platinum.
- other catalytic particles can be used as well.
- a variety of different solvents can be used as well, including, but not limited to, water, cyclohexane, and toluene.
- the particles and the solvent are mixed via some form of agitation.
- shear mixing is used to mix the particles and the solvent.
- sonication is used to mix the particles and the solvent.
- a size distribution analysis is performed on a sample of the particle-solvent mixture. This analysis results in the determination of a size distribution profile for the particle-solvent mixture.
- this size distribution analysis comprises centrifuging the sample of the particle-solvent mixture, and performing a Dynamic Light Scattering (DLS) process on the centrifuged sample. If the size distribution profile of the sample is below a predetermined threshold, then the catalytic particles and the solvent in the particle-solvent mixture are mixed again at step 110 , as shown by the dotted arrow.
- DLS Dynamic Light Scattering
- the entire particle-solvent mixture is centrifuged at step 130 , thereby forming a supernate of the particle-solvent mixture and a precipitate of the particle-solvent mixture within the same container.
- the supernate comprises a dispersion that includes the catalytic particles and the solvent.
- step 140 the particle-solvent mixture is decanted. This decanting step separates the supernate from the precipitate.
- the particle content of a sample of the separated supernate is determined.
- this particle content determination comprises performing a weight percentage calculation of the catalytic particles in the separated dispersion.
- this particle content determination comprises performing an Inductively Coupled Plasma Mass Spectrometry (ICP-MS) process on the separated dispersion.
- this particle content determination comprises performing both the weight percentage calculation and the ICP-MS process.
- the process goes back to the beginning if the particle content does not meet a predetermined threshold, as shown by the dotted arrow.
- additional catalytic particles are added to and mixed with the dispersion at step 110 if the particle content does not meet a predetermined threshold.
- completely new particles and solvent are used to form a completely new dispersion.
- a target volume of the dispersion to be applied to a catalyst support is determined based on one or more properties of the catalyst support.
- properties include, but are not limited to, the size of the support, the shape of the support, and the type of support (e.g., whether it is an extrudate, a powder, or a monolith).
- the catalyst support is impregnated with the catalytic particles in the dispersion. This impregnation is accomplished by applying the target volume of the dispersion to the catalyst support. In some embodiments, the application of the dispersion to the catalyst support is repeated in order to sufficiently impregnate the support. In some embodiments, this repetition is predetermined by the previously determined particle content of the supernate and/or properties of the catalyst support.
- the process continues to step 180 , where the impregnated catalyst support is calcined. It has been found to be advantageous for calcination to be performed between 350 degrees Celsius and 550 degrees Celsius for one to three hours. However, other temperatures and times can be employed as well, with variance of the temperature and time depending on the properties of the catalytic particles and/or the catalyst support.
- the impregnated catalyst support is analyzed to determine if it has been sufficiently impregnated according to one or more predetermined thresholds.
- this analysis comprises performing an Inductively Coupled Plasma Mass Spectrometry (ICP-MS) process on the impregnated catalyst support.
- ICP-MS Inductively Coupled Plasma Mass Spectrometry
- the process repeats the impregnation of the catalyst support at step 170 if the threshold is not met. In some embodiments, such repetition of the impregnation step requires determining the appropriate volume of the dispersion to be applied to the catalyst support at step 160 . If the threshold is met, then the catalyst has been properly produced and the process comes to an end.
- FIG. 2A illustrates one embodiment of a method 200 a of producing a dispersion in accordance with the principles of the present invention.
- FIG. 2A provides a more detailed embodiment of steps 110 to 150 of FIG. 1 . Accordingly, method 200 a comprises all of the features discussed above with respect to FIG. 1 .
- an incoming powder is provided.
- the powder comprises catalytic particles.
- the powder consists only of catalytic particles.
- the powder can either be stored and handled in an ambient environment or in an inert environment.
- the powder goes through ambient storage.
- the powder may be placed in a bottle on a shelf.
- the powder is then weighed at a weight station at step 206 a .
- a solvent bench is then used to add solvent to the powder at step 208 a .
- Steps 206 a and 208 a occur in open air.
- the powder goes through inert storage at step 204 b .
- a desired quantity of the powder is weighed at a weigh station at step 206 b .
- a solvent bench is then used to add solvent to the powder at step 208 b .
- Steps 206 b and 208 b occur in an inert environment in a dry box or glove box.
- a noble gas such as argon, is introduced into the box to create and maintain a very high purity inert atmosphere within the box. This inert atmosphere is particularly helpful in handling titanium carbide or pure metal powder.
- the powder and the solvent that were introduced to each other at step 208 are mixed together using a shear mixer, thereby producing a particle-solvent mixture.
- the powder and the solvent can be mixed together using other forms of agitation as well.
- the powder and the solvent are mixed together using sonication.
- the particle-solvent mixture is put through DLS staging in order to determine the dispersion quality of the particle-solvent mixture.
- a sample is pulled from the mixture.
- the sample is centrifuged.
- a DLS test is performed on the centrifuged sample in order to determine the size distribution of the small particles in the mixture.
- the data from the DLS test is recorded.
- it is determined whether or not the dispersion quality of the sample is sufficient. If the dispersion quality is not sufficient, then the process repeats the mixing step at 210 in order to improve the size distribution of the small particles.
- step 214 the entire vat of the dispersion mixture is put into a large centrifuge, which rapidly ages the dispersion.
- the mixture is spun at about 2500 rpms. All of the large particles settle to the bottom in pellet form, thereby resulting in a supernate that is a good dispersion and that is going to remain stable for numerous days to weeks.
- the supernate is decanted off, thereby removing the good dispersion from the large precipitate.
- the precipitate is treated as solid waste. In some embodiments, the precipitate is trashed at step 220 if it is a non-precious metal and reclaimed at step 222 if it is a precious metal.
- the decanted supernate is used as the dispersion for the rest of the process.
- a sample of the dispersion is pulled.
- the sample is then dried down at step 228 , which allows for the calculation of the weight percentage of the catalytic particles in the sample at step 230 .
- an ICP-MS process is performed on the sample at step 240 .
- the ICP-MS process determines the total metal content in the dispersion.
- step 232 it is determined whether or not the calculated weight percentage is sufficient. If the weight percentage is not sufficient, then the process starts over at one of the powder weighing steps at 206 a or 206 b . If the weight percentage is sufficient, then the process continues on to formation of the catalyst shown in FIG. 2B . In some embodiments, if the weight percentage is sufficient, then the powder goes to the shipping department at step 238 . In some embodiments, the pulled sample is disposed of at step 236 no matter what the determination is at step 232 , i.e., whether or not the weight percentage is sufficient.
- FIG. 2B illustrates one embodiment of a method 200 b of impregnating a catalyst support with particles from a dispersion in accordance with the principles of the present invention.
- FIG. 2B provides a more detailed embodiment of steps 160 to 190 of FIG. 1 .
- method 200 b comprises all of the features discussed above with respect to FIG. 1 . Additionally, it is contemplated that, in some embodiments, the steps of method 200 b are performed in an inert environment where possible with the dispersion being inertly stored.
- a catalyst support is selected to receive the catalytic particles from the dispersion produced in FIG. 2A .
- the catalytic particles will either be impregnated onto a porous extrudate, coated onto a micron powder or macro powder of sorts, or coated onto a monolith.
- an extrudate is selected to act ast the catalyst support.
- Different extrudates have different internal volumes and different pore sizes. Therefore, it is important to know the internal volume in order to calculate how much dispersion to add into the extrudate at step 246 . For example, if it is determined that an extrudate has an internal volume of 0.52 ml per gram and that there is 100 grams of extrudate material, then it can be determined exactly how much dispersion to add to the extrudate in order take up the entire pore space. If you add any more than the determined amount, then you are past the incipient wetness. If you add any less, then you are not accessing all of the possible pores. Therefore, it is important to add just the right amount of the dispersion.
- the extrudate is impregnated with the catalytic particles of the dispersion. It is contemplated that the impregnation of the extrudate can be performed in a variety of ways.
- one or more extrudates are placed in a laboratory flask that has a first neck with an opening and a second neck with an opening.
- a rubber stopper is used to seal the opening of the first neck, while a vacuum pump is hooked up to the opening of the second neck.
- a vacuum is pulled on the extrudates in the flask down to approximately less than 500 microns. In some embodiments, the vacuum is pulled for a time between approximately 10 minutes and approximately 20 minutes, depending on how many extrudates are in the flask and their total mass.
- Pulling the vacuum on the extrudates gets the interior volume of the flask down to a certain pressure that enables a rapid impregnation. Pulling a vacuum removes all of the air from the internal pores of the extrudates, which allows a liquid to penetrate the pores more rapidly. As a result of pulling the vacuum, we are left with one or more dry extrudates sitting at the bottom of the flask. The vacuum is closed off, such as through the use of one or more valves.
- a syringe is used to inject the previously determined volume of dispersion into the flask. In some embodiments, the syringe is used to puncture the rubber stopper and then to inject the dispersion. Preferably, no action is performed on the extrudates for 10 to 15 minutes in order to make sure that the entire extrudate has the opportunity to be impregnated.
- a freeze-drying process is performed on the impregnated catalyst support. If the flask discussed above is used, then the vacuum is broken by pulling the rubber septum off. Liquid nitrogen is poured into the flask, which is different from what is traditionally done.
- liquid nitrogen is poured into the flask, letting everything freeze. Then, all of the liquid nitrogen is allowed to boil off into nitrogen.
- the flask is hooked up to a freeze dryer.
- the freeze dryer is just a strong pump that pulls strong enough to keep the material inside the flask frozen. It pulls all of the solvent, such as water in most cases, directly past the cold finger (at ⁇ 50 to ⁇ 80 degrees Celsius) so that all of the vapor condenses off of the cold finger in order to avoid any damage to the pump.
- step 252 it is determined whether or not the impregnation should be repeated. For example, if you need a highly loaded catalyst (e.g., 10% platinum) on the extrudate, you might have to repeat the impregnation process a couple of times because the dispersion might not be as concentrated as it needs to be to require only one exposure. In some embodiments, this determination is based on the ICP-MS process performed at step 240 . If it is determined that another impregnation is required, then the process repeats the impregnation at step 248 . In some embodiments, a volume of dispersion is calculated once again at step 246 before proceeding to the impregnation step 248 .
- a highly loaded catalyst e.g. 10% platinum
- the impregnated extrudates are calcined at step 254 .
- the calcination step is a hardening step, performed to adhere the catalytic particles to the support. Calcination preferably occurs between 350 and 550 degrees Celsius for 1 to 3 hours. Depending on the type of metal, the temperature and the heating time can be varied.
- an ICP-MS process is performed on a sample of the impregnated extrudate in order to get elemental analysis on it and to make sure that there is sufficient loading.
- a powder or a monolith is used as the catalyst support at step 262 .
- step 264 after massing out a certain amount of powder or the monolith that you want coated with the catalytic particles, you calculate the volume that you need to sufficiently impregnate the support, similar to step 246 .
- this dispersion comprises catalytic nano-particles dispersed in a liquid. That dispersion is mixed with the support, whether it be a macro support, a micron powder, or a monolith. This mixing step serves to impregnate the support with the catalytic particles.
- a freeze-drying process is performed on the impregnated support, such as in step 250 .
- other drying processes can be used instead of freeze-drying, such as hot drying or flash drying.
- a hot drying process comprises any way to remove the solvent at a temperature greater than room temperature, but not hotter than the calcining temperature. For example, if you want to remove water, you can use a hot drying step at 110 degrees Celsius at ambient pressure and just let it bake for 1 to 2 hours until the material is dry.
- a flash drying process comprises anything that removes the solvent at a temperature that is as hot or hotter than the calcining temperature. For example, a furnace can be set at 550 degrees Celsius. The impregnated mixture is then placed into the furnace.
- the hot drying process or the flash drying process is used in place of the freeze-drying process at step 250 and/or at step 268 .
- the support is calcined, as in step 254 .
- An ICP-MS process is then performed on a sample of the support at step 272 in order to get elemental analysis on it and to make sure that there is sufficient loading.
- one or more properties of the catalyst support are used in order to determine the proper amount of dispersion to use in impregnating the support. Determining the internal volume of the extrudate is particularly useful, as you do not want to use any more or any less dispersion than that internal volume. If you use any more than that internal volume, then you risk capillary forces drawing material out of the extrudate. If you use any less than that internal volume, then you are not accessing all of the pores, and therefore, not giving yourself the best chance of impregnation. The present invention also uses the ICP-MS process before the impregnation steps in order to determine the appropriate number of impregnations to be performed.
- the monolith is dipped into the dispersion, but a freeze-drying process is not used. Instead, a hot drying process or a flash drying process is used.
- impregnated extrudates can be used to impregnate a monolith. For example, if it is determined at step 258 that there is sufficient loading on the extrudates, then these impregnated extrudates can be used to impregnate a monolith, since the extrudates are coated with catalytic particles on the inside.
- the extrudates are crushed up into powder (e.g., 10 micron powder or 40 micron powder). This crushed up powder contains the catalytic particles. The powder is then put into a slurry, which is used to coat the monolith.
Abstract
Description
- This application claims priority to U.S. Provisional Patent Application Ser. No. 61/284,329, filed Dec. 15, 2009 and entitled “MATERIALS PROCESSING,” which is hereby incorporated herein by reference in its entirety as if set forth herein.
- The present invention relates to the field of catalysts. More specifically, the present invention relates to a method of producing a catalyst.
- In one aspect of the present invention, a method of producing a catalyst is provided. The method comprises mixing a plurality of catalytic particles and a solvent, thereby forming a particle-solvent mixture. A size distribution analysis is performed on a sample of the particle-solvent mixture, thereby determining a size distribution profile for the particle-solvent mixture. The mixing of the catalytic particles and the solvent in the particle-solvent mixture is repeated if the size distribution profile is below a predetermined threshold. The entire particle-solvent mixture is centrifuged if the size distribution profile is at or above the predetermined threshold, thereby forming a supernate of the particle-solvent mixture and a precipitate of the particle-solvent mixture within the same container, wherein the supernate comprises a dispersion including the catalytic particles and the solvent. The particle-solvent mixture is decanted, thereby separating the supernate from the precipitate. The particle content of a sample of the separated supernate is determined. A target volume of the dispersion to be applied to a catalyst support is determined based on one or more properties of the catalyst support. The catalyst support is impregnated with the catalytic particles in the dispersion by applying the target volume of the dispersion to the catalyst support.
- In some embodiments, the method further comprises the step of calcining the impregnated catalyst support. In some embodiments, the method further comprises the step of performing a drying process on the impregnated catalyst support before the step of calcining the impregnated catalyst support. In some embodiments, the drying process is a freeze drying process.
- In some embodiments, the method further comprises the step of analyzing the impregnated catalyst support to determine if it has been sufficiently impregnated according to one or more predetermined thresholds. In some embodiments, the step of analyzing the impregnated catalyst support comprises performing an Inductively Coupled Plasma Mass Spectrometry (ICP-MS) process on the impregnated catalyst support. In some embodiments, the method further comprises the step of performing an additional impregnation of the impregnated catalyst support with a dispersion of catalytic particles in response to a determination by the analyzing step that the impregnated catalyst support has not been sufficiently impregnated according to the one or more thresholds.
- In some embodiments, the catalyst support is a porous extrudate. In some embodiments, the catalyst support is a monolith. In some embodiments, the catalyst support is a powder.
- In some embodiments, the step of mixing the plurality of catalytic particles and the solvent comprises using a shear mixer to mix the plurality of catalytic particles and the solvent. In some embodiments, the step of mixing the plurality of catalytic particles and the solvent comprises using sonication to mix the plurality of catalytic particles and the solvent.
- In some embodiments, the step of performing a size distribution analysis on the sample of the particle-solvent mixture comprises: centrifuging the sample of the particle-solvent mixture; and performing a Dynamic Light Scattering (DLS) process on the centrifuged sample.
- In some embodiments, the step of determining the particle content of the sample of the separated supernate comprises calculating the weight percentage of the catalytic particles in the sample. In some embodiments, the step of determining the particle content of the sample of the separated supernate comprises performing an Inductively Coupled Plasma Mass Spectrometry (ICP-MS) process on the sample.
- In some embodiments, the plurality of catalytic particles that is mixed with the solvent is a nano-powder.
- In another aspect of the present invention, a method of producing a catalyst is provided. The method comprises mixing a plurality of catalytic particles and a solvent, thereby forming a particle-solvent mixture. A sample of the particle-solvent mixture is centrifuged. A Dynamic Light Scattering (DLS) process is performed on the centrifuged sample, thereby determining a size distribution profile for the particle-solvent mixture. The mixing of the catalytic particles and the solvent in the particle-solvent mixture is repeated if the size distribution profile is below a predetermined threshold. The entire particle-solvent mixture is centrifuged if the size distribution profile is at or above the predetermined threshold, thereby forming a supernate of the particle-solvent mixture and a precipitate of the particle-solvent mixture within the same container, wherein the supernate comprises a dispersion including the catalytic particles and the solvent. The particle-solvent mixture is decanted, thereby separating the supernate from the precipitate. The catalyst support is impregnated with the catalytic particles in the dispersion by applying a volume of the dispersion to the catalyst support.
- In some embodiments, the method further comprises performing a dry-down process on a sample of the separated dispersion, and performing a weight percentage calculation of the catalytic particles using the dried-down sample of the separated dispersion, thereby determining a weight percentage for the catalytic particles. In some embodiments, the step of impregnating the catalyst support is performed only if the determined weight percentage for the catalytic particles is at or above a predetermined threshold. In some embodiments, an Inductively Coupled Plasma Mass Spectrometry (ICP-MS) process is performed on the dried-down sample of the separated dispersion.
- In yet another aspect of the present invention, a method of producing a catalyst is provided. The method comprises providing a dispersion, wherein the dispersion comprises catalytic particles dispersed in a solvent. A target volume of the dispersion to be applied to a catalyst support is determined based on one or more properties of the catalyst support. The catalyst support is impregnated with the catalytic particles in the dispersion by applying the target volume of the dispersion to the catalyst support. A drying process is performed on the impregnated catalyst support. The dried impregnated catalyst support is calcined. An Inductively Coupled Plasma Mass Spectrometry (ICP-MS) process is performed on the calcined impregnated catalyst support to determine if it has been sufficiently impregnated according to one or more predetermined thresholds. An additional impregnation of the impregnated catalyst support with a dispersion of catalytic particles is performed if it is determined by the ICP-MS process that the impregnated catalyst support has not been sufficiently impregnated according to the one or more thresholds.
- In some embodiments, the catalyst support is a porous extrudate. In some embodiments, the catalyst support is a monolith. In some embodiments, the catalyst support is a powder.
- In some embodiments, the drying process is a freeze drying process. In some embodiments, the drying process is either a hot drying process or a flash drying process.
-
FIG. 1 illustrates one embodiment of a method of producing a catalyst in accordance with the principles of the present invention. -
FIG. 2A illustrates one embodiment of a method of producing a dispersion in accordance with the principles of the present invention. -
FIG. 2B illustrates one embodiment of a method of impregnating a catalyst support with particles from a dispersion in accordance with the principles of the present invention. - The following description is presented to enable one of ordinary skill in the art to make and use the invention and is provided in the context of a patent application and its requirements. Various modifications to the described embodiments will be readily apparent to those skilled in the art and the generic principles herein may be applied to other embodiments. Thus, the present invention is not intended to be limited to the embodiment shown but is to be accorded the widest scope consistent with the principles and features described herein.
- This disclosure refers to both particles and powders. These two terms are equivalent, except for the caveat that a singular “powder” refers to a collection of particles. The present invention may apply to a wide variety of powders and particles. Powders that fall within the scope of the present invention may include, but are not limited to, any of the following: (a) nano-structured powders (nano-powders), having an average grain size less than 250 nanometers and an aspect ratio between one and one million; (b) submicron powders, having an average grain size less than 1 micron and an aspect ratio between one and one million; (c) ultra-fine powders, having an average grain size less than 100 microns and an aspect ratio between one and one million; and (d) fine powders, having an average grain size less than 500 microns and an aspect ratio between one and one million.
- Various aspects of the disclosure may be described through the use of flowcharts. Often, a single instance of an aspect of the present disclosure may be shown. As is appreciated by those of ordinary skill in the art, however, the protocols, processes, and procedures described herein may be repeated continuously or as often as necessary to satisfy the needs described herein. Additionally, it is contemplated that certain method steps of the invention can be performed in alternative sequences to those disclosed in the flowcharts. Accordingly, the scope of the claims should not be limited to any specific order of method steps unless the order is explicitly required by the language of the claims.
-
FIG. 1 illustrates one embodiment of amethod 100 of producing a catalyst in accordance with the principles of the present invention. - At
step 110, a plurality of catalytic particles and a solvent are mixed together, thereby forming a particle-solvent mixture. It is contemplated that the catalytic particles can be made up of any particles having catalytic properties such that they modify, either by increasing or decreasing, the rate of a chemical reaction. In some embodiments, the catalytic particles comprise or consist of one or more precious metals. In some embodiments, the catalytic particles comprise one of the platinum group metals, such as ruthenium, rhodium, palladium, osmium, iridium, and platinum. However, other catalytic particles can be used as well. A variety of different solvents can be used as well, including, but not limited to, water, cyclohexane, and toluene. In a preferred embodiment, the particles and the solvent are mixed via some form of agitation. In some embodiments, shear mixing is used to mix the particles and the solvent. In some embodiments, sonication is used to mix the particles and the solvent. - At
step 120, a size distribution analysis is performed on a sample of the particle-solvent mixture. This analysis results in the determination of a size distribution profile for the particle-solvent mixture. In some embodiments, this size distribution analysis comprises centrifuging the sample of the particle-solvent mixture, and performing a Dynamic Light Scattering (DLS) process on the centrifuged sample. If the size distribution profile of the sample is below a predetermined threshold, then the catalytic particles and the solvent in the particle-solvent mixture are mixed again atstep 110, as shown by the dotted arrow. - Once the size distribution profile is at or above the predetermined threshold (whether it is after the original mixing step or after subsequent repeated mixing steps) the entire particle-solvent mixture is centrifuged at
step 130, thereby forming a supernate of the particle-solvent mixture and a precipitate of the particle-solvent mixture within the same container. The supernate comprises a dispersion that includes the catalytic particles and the solvent. - At
step 140, the particle-solvent mixture is decanted. This decanting step separates the supernate from the precipitate. - At
step 150, the particle content of a sample of the separated supernate is determined. In some embodiments, this particle content determination comprises performing a weight percentage calculation of the catalytic particles in the separated dispersion. In some embodiments, this particle content determination comprises performing an Inductively Coupled Plasma Mass Spectrometry (ICP-MS) process on the separated dispersion. In some embodiments, this particle content determination comprises performing both the weight percentage calculation and the ICP-MS process. In some embodiments, the process goes back to the beginning if the particle content does not meet a predetermined threshold, as shown by the dotted arrow. In some embodiments, additional catalytic particles are added to and mixed with the dispersion atstep 110 if the particle content does not meet a predetermined threshold. In some embodiments, completely new particles and solvent are used to form a completely new dispersion. - At
step 160, a target volume of the dispersion to be applied to a catalyst support is determined based on one or more properties of the catalyst support. Such properties include, but are not limited to, the size of the support, the shape of the support, and the type of support (e.g., whether it is an extrudate, a powder, or a monolith). - At
step 170, the catalyst support is impregnated with the catalytic particles in the dispersion. This impregnation is accomplished by applying the target volume of the dispersion to the catalyst support. In some embodiments, the application of the dispersion to the catalyst support is repeated in order to sufficiently impregnate the support. In some embodiments, this repetition is predetermined by the previously determined particle content of the supernate and/or properties of the catalyst support. - In some embodiments, the process continues to step 180, where the impregnated catalyst support is calcined. It has been found to be advantageous for calcination to be performed between 350 degrees Celsius and 550 degrees Celsius for one to three hours. However, other temperatures and times can be employed as well, with variance of the temperature and time depending on the properties of the catalytic particles and/or the catalyst support.
- At
step 190, the impregnated catalyst support is analyzed to determine if it has been sufficiently impregnated according to one or more predetermined thresholds. In some embodiments, this analysis comprises performing an Inductively Coupled Plasma Mass Spectrometry (ICP-MS) process on the impregnated catalyst support. In some embodiments, the process repeats the impregnation of the catalyst support atstep 170 if the threshold is not met. In some embodiments, such repetition of the impregnation step requires determining the appropriate volume of the dispersion to be applied to the catalyst support atstep 160. If the threshold is met, then the catalyst has been properly produced and the process comes to an end. -
FIG. 2A illustrates one embodiment of amethod 200 a of producing a dispersion in accordance with the principles of the present invention.FIG. 2A provides a more detailed embodiment ofsteps 110 to 150 ofFIG. 1 . Accordingly,method 200 a comprises all of the features discussed above with respect toFIG. 1 . - At
step 202, an incoming powder is provided. In a preferred embodiment, the powder comprises catalytic particles. In some embodiments, the powder consists only of catalytic particles. The powder can either be stored and handled in an ambient environment or in an inert environment. - At
step 204 a, the powder goes through ambient storage. For example, the powder may be placed in a bottle on a shelf. The powder is then weighed at a weight station atstep 206 a. A solvent bench is then used to add solvent to the powder atstep 208 a.Steps - Alternatively, the powder goes through inert storage at
step 204 b. A desired quantity of the powder is weighed at a weigh station atstep 206 b. A solvent bench is then used to add solvent to the powder atstep 208 b.Steps - At step 210, the powder and the solvent that were introduced to each other at step 208 are mixed together using a shear mixer, thereby producing a particle-solvent mixture. As previously mentioned, the powder and the solvent can be mixed together using other forms of agitation as well. In some embodiments, the powder and the solvent are mixed together using sonication.
- At
step 212, the particle-solvent mixture is put through DLS staging in order to determine the dispersion quality of the particle-solvent mixture. At step 212-1 of the DLS staging, a sample is pulled from the mixture. At step 212-2 of the DLS staging, the sample is centrifuged. At step 212-3 of the DLS staging, a DLS test is performed on the centrifuged sample in order to determine the size distribution of the small particles in the mixture. At step 212-4, the data from the DLS test is recorded. At step 212-5, it is determined whether or not the dispersion quality of the sample is sufficient. If the dispersion quality is not sufficient, then the process repeats the mixing step at 210 in order to improve the size distribution of the small particles. - If the dispersion quality is sufficient, then the process continues to step 214, where the entire vat of the dispersion mixture is put into a large centrifuge, which rapidly ages the dispersion. In a preferred embodiment, the mixture is spun at about 2500 rpms. All of the large particles settle to the bottom in pellet form, thereby resulting in a supernate that is a good dispersion and that is going to remain stable for numerous days to weeks.
- At
step 216, the supernate is decanted off, thereby removing the good dispersion from the large precipitate. Atstep 218, the precipitate is treated as solid waste. In some embodiments, the precipitate is trashed atstep 220 if it is a non-precious metal and reclaimed atstep 222 if it is a precious metal. - At
step 224, the decanted supernate is used as the dispersion for the rest of the process. Atstep 226, a sample of the dispersion is pulled. The sample is then dried down atstep 228, which allows for the calculation of the weight percentage of the catalytic particles in the sample atstep 230. In the middle of getting the dry down, an ICP-MS process is performed on the sample atstep 240. The ICP-MS process determines the total metal content in the dispersion. - At
step 232, it is determined whether or not the calculated weight percentage is sufficient. If the weight percentage is not sufficient, then the process starts over at one of the powder weighing steps at 206 a or 206 b. If the weight percentage is sufficient, then the process continues on to formation of the catalyst shown inFIG. 2B . In some embodiments, if the weight percentage is sufficient, then the powder goes to the shipping department at step 238. In some embodiments, the pulled sample is disposed of atstep 236 no matter what the determination is atstep 232, i.e., whether or not the weight percentage is sufficient. -
FIG. 2B illustrates one embodiment of amethod 200 b of impregnating a catalyst support with particles from a dispersion in accordance with the principles of the present invention.FIG. 2B provides a more detailed embodiment ofsteps 160 to 190 ofFIG. 1 . Accordingly,method 200 b comprises all of the features discussed above with respect toFIG. 1 . Additionally, it is contemplated that, in some embodiments, the steps ofmethod 200 b are performed in an inert environment where possible with the dispersion being inertly stored. - At
step 242, a catalyst support is selected to receive the catalytic particles from the dispersion produced inFIG. 2A . In some embodiments, the catalytic particles will either be impregnated onto a porous extrudate, coated onto a micron powder or macro powder of sorts, or coated onto a monolith. - At
step 244, an extrudate is selected to act ast the catalyst support. Different extrudates have different internal volumes and different pore sizes. Therefore, it is important to know the internal volume in order to calculate how much dispersion to add into the extrudate atstep 246. For example, if it is determined that an extrudate has an internal volume of 0.52 ml per gram and that there is 100 grams of extrudate material, then it can be determined exactly how much dispersion to add to the extrudate in order take up the entire pore space. If you add any more than the determined amount, then you are past the incipient wetness. If you add any less, then you are not accessing all of the possible pores. Therefore, it is important to add just the right amount of the dispersion. - At
step 248, the extrudate is impregnated with the catalytic particles of the dispersion. It is contemplated that the impregnation of the extrudate can be performed in a variety of ways. In some embodiments, one or more extrudates are placed in a laboratory flask that has a first neck with an opening and a second neck with an opening. A rubber stopper is used to seal the opening of the first neck, while a vacuum pump is hooked up to the opening of the second neck. A vacuum is pulled on the extrudates in the flask down to approximately less than 500 microns. In some embodiments, the vacuum is pulled for a time between approximately 10 minutes and approximately 20 minutes, depending on how many extrudates are in the flask and their total mass. Pulling the vacuum on the extrudates gets the interior volume of the flask down to a certain pressure that enables a rapid impregnation. Pulling a vacuum removes all of the air from the internal pores of the extrudates, which allows a liquid to penetrate the pores more rapidly. As a result of pulling the vacuum, we are left with one or more dry extrudates sitting at the bottom of the flask. The vacuum is closed off, such as through the use of one or more valves. A syringe is used to inject the previously determined volume of dispersion into the flask. In some embodiments, the syringe is used to puncture the rubber stopper and then to inject the dispersion. Preferably, no action is performed on the extrudates for 10 to 15 minutes in order to make sure that the entire extrudate has the opportunity to be impregnated. - Different techniques can be used depending on what you want the end product to be. For example, if you want an eggshell extrudate where it is mostly coating on the outside, you can break the vacuum quickly or you can avoid pulling the vacuum at all. If you want to make sure that there is uniform coating all the way to the interior of the extrudate, you can let it sit a little bit longer to make sure that the entire extrudate has a chance to be impregnated.
- At
step 250, a freeze-drying process is performed on the impregnated catalyst support. If the flask discussed above is used, then the vacuum is broken by pulling the rubber septum off. Liquid nitrogen is poured into the flask, which is different from what is traditionally done. - Traditionally, if you want to freeze dry something, you start off with a liquid in a flask and put it into a dewar of liquid nitrogen. You try to create as much surface area as you freeze the material on the inside of the flask. Once it is frozen, you hook it up to a freeze dryer. However, since you have a lot of liquid that is on the interior of these extrudates, you cannot freeze them very quickly by just setting the flask into a liquid nitrogen dewar. It takes too long.
- Instead, in the present invention, liquid nitrogen is poured into the flask, letting everything freeze. Then, all of the liquid nitrogen is allowed to boil off into nitrogen. When there is no more liquid in the flask, the flask is hooked up to a freeze dryer. In some embodiments, the freeze dryer is just a strong pump that pulls strong enough to keep the material inside the flask frozen. It pulls all of the solvent, such as water in most cases, directly past the cold finger (at −50 to −80 degrees Celsius) so that all of the vapor condenses off of the cold finger in order to avoid any damage to the pump.
- It is important to pull a strong enough vacuum to keep the material inside the flask frozen. The sublimation rate has to be that at which the material stays frozen throughout the entire process. In order to make sure that happens, when you first start off with the freeze drying, usually you insulate the flask a little bit and let a strong vacuum be pulled on it. As you notice the flask not being as cold as it used to be, you start removing a little bit of insulation. It is all finished when you still have that strong of a vacuum and your flask is at room temperature so you know that nothing else can be sublimed.
- At step 252, it is determined whether or not the impregnation should be repeated. For example, if you need a highly loaded catalyst (e.g., 10% platinum) on the extrudate, you might have to repeat the impregnation process a couple of times because the dispersion might not be as concentrated as it needs to be to require only one exposure. In some embodiments, this determination is based on the ICP-MS process performed at
step 240. If it is determined that another impregnation is required, then the process repeats the impregnation atstep 248. In some embodiments, a volume of dispersion is calculated once again atstep 246 before proceeding to theimpregnation step 248. - If it is determined that another impregnation is not required, then the impregnated extrudates are calcined at
step 254. At this stage, the extrudates are already dry. The calcination step is a hardening step, performed to adhere the catalytic particles to the support. Calcination preferably occurs between 350 and 550 degrees Celsius for 1 to 3 hours. Depending on the type of metal, the temperature and the heating time can be varied. - At step 256, an ICP-MS process is performed on a sample of the impregnated extrudate in order to get elemental analysis on it and to make sure that there is sufficient loading. At
step 258, it is determined whether or not there is sufficient loading on the catalyst support. If there is not sufficient loading, then the process repeats the impregnation of the support atstep 248. If there is sufficient loading, then the impregnated supports go to the shipping department atstep 260. - In some embodiments, instead of an extrudate, a powder or a monolith is used as the catalyst support at
step 262. Atstep 264, after massing out a certain amount of powder or the monolith that you want coated with the catalytic particles, you calculate the volume that you need to sufficiently impregnate the support, similar to step 246. - At
step 266, you mix the support with a second component, which is the dispersion. In some embodiments, this dispersion comprises catalytic nano-particles dispersed in a liquid. That dispersion is mixed with the support, whether it be a macro support, a micron powder, or a monolith. This mixing step serves to impregnate the support with the catalytic particles. - At
step 268, a freeze-drying process is performed on the impregnated support, such as instep 250. However, it is contemplated that other drying processes can be used instead of freeze-drying, such as hot drying or flash drying. A hot drying process comprises any way to remove the solvent at a temperature greater than room temperature, but not hotter than the calcining temperature. For example, if you want to remove water, you can use a hot drying step at 110 degrees Celsius at ambient pressure and just let it bake for 1 to 2 hours until the material is dry. A flash drying process comprises anything that removes the solvent at a temperature that is as hot or hotter than the calcining temperature. For example, a furnace can be set at 550 degrees Celsius. The impregnated mixture is then placed into the furnace. The solvent evaporates quick enough so that you limit the capillary forces of the solvent evaporating, allowing you to freeze material in that spot or secure material in that location more readily than you can if you use a slow hot drying process. In some embodiments, the hot drying process or the flash drying process is used in place of the freeze-drying process atstep 250 and/or atstep 268. - At
step 270, the support is calcined, as instep 254. An ICP-MS process is then performed on a sample of the support atstep 272 in order to get elemental analysis on it and to make sure that there is sufficient loading. Atstep 274, it is determined whether or not there is sufficient loading on the catalyst support. If there is not sufficient loading, then the process repeats the impregnation of the support. In some embodiments, this repeated impregnation begins with a recalculation of the volume needed to sufficiently impregnate the support atstep 264. In some embodiments, the repeated impregnation step goes directly to the mixing of the support with a volume of the dispersion atstep 266. If there is sufficient loading, then the impregnated supports go to the shipping department atstep 260. - In the present invention, one or more properties of the catalyst support are used in order to determine the proper amount of dispersion to use in impregnating the support. Determining the internal volume of the extrudate is particularly useful, as you do not want to use any more or any less dispersion than that internal volume. If you use any more than that internal volume, then you risk capillary forces drawing material out of the extrudate. If you use any less than that internal volume, then you are not accessing all of the pores, and therefore, not giving yourself the best chance of impregnation. The present invention also uses the ICP-MS process before the impregnation steps in order to determine the appropriate number of impregnations to be performed.
- In some embodiments where a ceramic monolith is used for the catalyst support, the monolith is dipped into the dispersion, but a freeze-drying process is not used. Instead, a hot drying process or a flash drying process is used.
- In some embodiments, impregnated extrudates can be used to impregnate a monolith. For example, if it is determined at
step 258 that there is sufficient loading on the extrudates, then these impregnated extrudates can be used to impregnate a monolith, since the extrudates are coated with catalytic particles on the inside. The extrudates are crushed up into powder (e.g., 10 micron powder or 40 micron powder). This crushed up powder contains the catalytic particles. The powder is then put into a slurry, which is used to coat the monolith. - The present invention has been described in terms of specific embodiments incorporating details to facilitate the understanding of principles of construction and operation of the invention. Such reference herein to specific embodiments and details thereof is not intended to limit the scope of the claims appended hereto. It will be readily apparent to one skilled in the art that other various modifications may be made in the embodiment chosen for illustration without departing from the spirit and scope of the invention as defined by the claims.
Claims (26)
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JP2012544686A JP5860813B2 (en) | 2009-12-15 | 2010-12-13 | Catalyst production method and system |
EP10838185.6A EP2512660A4 (en) | 2009-12-15 | 2010-12-13 | Catalyst production method and system |
BR112012014424A BR112012014424A2 (en) | 2009-12-15 | 2010-12-13 | catalyst production method and system |
KR1020127018434A KR20120112562A (en) | 2009-12-15 | 2010-12-13 | Catalyst production method and system |
AU2010332042A AU2010332042B2 (en) | 2009-12-15 | 2010-12-13 | Catalyst production method and system |
MX2012006992A MX343636B (en) | 2009-12-15 | 2010-12-13 | Catalyst production method and system. |
CN201080063826.2A CN102834173B (en) | 2009-12-15 | 2010-12-13 | Method for preparing catalyst and system |
CA2784449A CA2784449A1 (en) | 2009-12-15 | 2010-12-13 | Catalyst production method and system |
PCT/US2010/060138 WO2011075447A1 (en) | 2009-12-15 | 2010-12-13 | Catalyst production method and system |
RU2012129985/04A RU2605415C2 (en) | 2009-12-15 | 2010-12-13 | Catalyst production method and system |
IL220391A IL220391A (en) | 2009-12-15 | 2012-06-13 | Catalyst production method and system |
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IL220391A0 (en) | 2012-08-30 |
EP2512660A4 (en) | 2014-10-01 |
RU2605415C2 (en) | 2016-12-20 |
CN102834173A (en) | 2012-12-19 |
EP2512660A1 (en) | 2012-10-24 |
CN102834173B (en) | 2015-08-05 |
US9149797B2 (en) | 2015-10-06 |
JP2013513485A (en) | 2013-04-22 |
IL220391A (en) | 2017-01-31 |
WO2011075447A1 (en) | 2011-06-23 |
JP5860813B2 (en) | 2016-02-16 |
AU2010332042A1 (en) | 2012-07-26 |
MX2012006992A (en) | 2012-11-23 |
MX343636B (en) | 2016-11-15 |
KR20120112562A (en) | 2012-10-11 |
CA2784449A1 (en) | 2011-06-23 |
BR112012014424A2 (en) | 2019-09-24 |
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AU2010332042B2 (en) | 2015-05-28 |
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